Production of polymerization products of diolefines



Fatented June '9, 1931 v V I I SAT'ES rArEr OFFICE CLAUS HEUCK AN D HANS ENDERLEIN, F LUDWIGSHAIEN -QN-THE-RHINE, GERMANY, ASSIGNORS TO I. G. FARBENINDUSTRIE AKTIENGESELLD'CHAFT, 0F ERANKFORT-O N- JPRQD'UCTION 0E POLYMEI R-IZATION PRODUCTS 01E DIOLEIFINES No Drawing. Application filed January 25, 1980, Serial No. 423,540, and index-many February 21, 1929.

This invention relates to improvements in a melting point of about 94.5 C. and comthe manufacture and production of polymerposed of about 8 partsof bismuth, parts ization products of diolefines. of lead and 3 parts of tin, or Roses alloy hav- J When removing non-distillable polymering a melting point of about 93.7 5 C. and ization products of diolefines such as butabeing composed of about 2 parts of bismuth, diene, isoprene or dimenthylbutadiene or -1 part of lead and 1 part of tin, there is a risk homologues and analogues thereof from the that the metal on melting penetrates the reaction vessels considerable diificulty is often polymerization product and can be removed encountered by reason of the fact that the retherefrom only with difliculty; this drawaction products adhere very firmly to the back is overcome by providing the metallic walls of the reaction vessels. surface with a lacquer coating.

We have now found that this difliculty is According to the present invention the obviated in a verysimple manner and that polymerization products are obtained in a the reaction products may be removed from form in which they may be readily taken out H the reaction vessels readily,rapidly and withfrom the vessel. The lining material which out leaving any residue, by lining or c0atin some cases adheres to the surface of the ing the reaction vessel with materials which product may be readily removed. When do not adhere to the walls of the vessel or paper, cardboard or the like has been emwhich may be readily removed therefrom, for ployed as the lining material, the reaction example which may be readily stripped ofi, product which'for example is coated with the 7 dissolved or melted away. lining material may be readily freed from For example the vessels may be coated with paper, cardboard or the like by immersion in linings of paper, cardboard, textile fabrics, water and slight mechanical treatment. The leather, sheet metal or with foils or films of removal of the lining material from the re- 25 cellulose derivatives or elastic or plastic action product may also be effected during polymerization products of diolefines or rubthe further working up of the product, if her, and the rubber or the said polymerizadesired. In many cases the removal of the v I tion products may have been vulcanized or lining material is not necessary, for example subsequently treated in any other way, or the When the polymerization of the diolefines has 30 vessels may be provided with a coating of been carried out with the employment of a so waxes, paraflin waxes, readily fusible metal lining of material which is not injurious in alloys or the like. It is frequently advanthe further working up of the product, 'for tageous to protect the layer which serves to example a lining of a polymerization product coat the vessel with a special layer before it of, a diolefine or a lining of a substance which 35 comes into contact with the contents of the has to be added to the polymerization prodv el- 7 not of the diolefine in the further working Thus, for example, when employing a linup of the same such as asphalt, zinc oxide, ng of waxy substances such as montan wax, carbon black and the like or mixtures of such araflin wax or bitumen, which are. soluble substances. I

40 in the butadiene, the lining must be coated The said olymerizationg may be carried with a substance which is insoluble in butaout in knownmanner, with the diolefines, for diene, for example with a nitrocellulose example, in an emulsified or dissolved state lacquer or a condensation product of urea or in' the undiluted liquid state or, in some and formaldehyde or a film of gelatine or cases, in the gaseous state.

45 casein. Also, when employing a lining of a The following examples will further illusreadily fusible metal such as Woods alloy, trate the nature of this invention but the inan alloy having a melting point of, about vention is not restricted thereto. 605 C. and 'being composed of about 4 parts E Z8 1 of bismuth, 2 parts of lead, 1 part of tin and mam? so 1 part of cadmium, or Newtons alloy having In order to prepare polymerization produ'cts of butadiene, a pressure autoclave of 150 liters capacity is provided with a lining of paper, for example a paper bag, and 50 kilograms of the butadiene are polymerized therein in the usual manner by heating for 3 days to about 50 C. with the addition of 0.5 kilogram of sodium as a catalyst. After the reaction has ended the polymerization product may be removed from the autoclave without difliculty. The adherent paper may be readily removed by soaking the polymerization product with water before or during the treatment on the rollers.

Ewampze 2 100 kilograms of butadiene and 2 kilograms of dimethyl-ether are filled into a revolving autoclave lined with Woods alloy and thereafter provided with a coating of a nitrocellulose lacquer or of gelatine. Polymerization is efiected, after the addition of 1 kilogram of sodium in the form of wire, by heating to from 50 polymerization is complete, the alloy is fused and withdrawn. The polymerization product can be removed from the autoclave wit h.

out difiiculty. The autoclave must be given a fresh lining with the alloy and coating before further use. i

Eazample 3 An autoclave of '30 liters capacity is lined with bitumen and the lining coated with water glass solution. After drying, the autoclave is filled with 15 liters of butadiene which is polymerized at from 50 to 60 C.

with the addition of 100 grams of sodium. After the polymerization is complete, the bitumen is melted. The polymerization product can be removed from the autoclave without difliculty. Depending on the purpose, for which it is to be used, the bitumen may remain with the polymerization prodnot, or it must be separated therefrom. I

What we claim is 1. In the polymerization of a diolefine to a non-distillable product, facilitating the re moval of the polymerization product from the reaction vessel by covering the inner wall of the reaction vessel with a sheet material a non-distillable product, facilitating the removal of the polymerization product from to 60 C. After the.

the reaction vessel by lining the walls of the reaction vessel with a paper bag.

In testimony whereof we have hereunto set our hands.

CLAUS HEUCK. HANS ENDERLEIN. 

